Method of producing salts of volatile bases.



v PATENTED MAY 21, 1907.

T. BLASS, J. L. HAEHNLEN 55 W. W. 00X.

METHOD OF PRODUCING SALTS 0F VOLATILE BASES.

APPLICATION FILED JULY 14, 1906.

2 SHEETS-SHEET 1.

- PATENTED MAY 21, 1907. T. BLASS, J. L. HAEHNLEN & W. w. 00X. METHOD. OF PRODUCING SALTS OF VOLATILB BASES.

APPLIOATION FILED JULY 14, 1906.

2 SHBETSSHEET 2.

nuanl'oz s $1 a; ma... Q Vihmase; I. W 5 4. 7K E9 i att'mug UNITED STATES PATENT OFFICE.

TALMADGE' BLASS, OF WEST SENECA, NEW YORK, AND JACOB LUTHER HAEHNLEN AND WALTER WETHERILL COX, OF LEBANON, PENNSYL- VANIA.

METHOD OF PRODUCING $ALTS OF VOLATlLE'BASES.

Specification of Letters Patent. Application filed July 14, 1906. Serial No. 326,281.

' United-States, have invented new and useful Improvements. in Methods of Producing Salts, of which the following is a specificati'on. v

Our invention relates to the manufacture of substantially pure salts, or what is known ,as l commercially pure salts, by the union of a volatile base with an acid radical, both being led in the gaseous'state into a suitable vessel where the base and acid radical combine and are'deposited in a powder as a salt; and

our invention more particularly relates tothe formation of ammonium sulfite and ammonium carbamate from furnace gases, as will be hereinafter more particularly described and claimed. 1

- Referring to the drawings, in which like parts are similarly designated: Figure 1 is an elevation, partly in section, of part of anapparatus designed to carry out our invention, and Fig. 2 is a like View forming a continuationof Fig. 1.

By a volatile base we Wish tobe understood to include any base like ammonium, such as lead, zinc, and the like, which, when broughtto a suitable temperature, will form a vapor or gas.

VVe have illustrated an apparatus suitable for carrying out our process, most of the parts of which are of well known construction, and particularly designed for the-distillation of ammonia and the formation of ammonium salts.

In the said drawings thereference numeral '2 denotes astorage tank for ammonia or ammonia liquor, such as is produced in the coking of coal. From this tank there is a pipe 3 having acut-ofi valve 4 extending over two elements of the plant, one of which is a preheater 5, andthe other a still 6, By closing the valved the liquor is delivered to the preheater, where it is heated to about 99 centiscribed in German patent to Solvay & 00., No. 49,500, dated November 4, 1888). The ammonia liquor is here freed from some of the sulfureted hydrogen, carbon dioXid and pyridene.

From the pre-heater the liquor is pumped by a centrifugal pump 7 to the still 6, where a certain quantity of ammonia liquor direct from tank 2 may or may not be united with it, as the exigencies of the operation and character of the product may require or demand. The still 6 maybe of any desired con-' struction, and I have shown the well known Feldman still. Ammonium gas is delivered from this still to a washer 8, also of well known construction, and is here freed from impurities, such as hydrogen sulfid, H 5, pyridene, cyanogen, etc. nected to washer 8 by pipe 9, and the ammo- Patented May 21, 1907.

The still 6 is 3011- nia gases are led from washer 8 by pipe. 10 1 and pipe 14 tothe combining chambers 15, 16, 17 and 18. Pipe 10 is providedwith a cut-off valve 11, and there is a by-pass 12 provided with a valve 13, by means, of which the gas may be delivered directly from the still 6 to pipe 14 and from thence to the combi'ning chambers.

A drip-tank 19 is designed to receive the drip from the washer 8, and the same is provided with a pipe 20 extending nearly to the bottom of said tank at one end and entering the pre-heater 5 at its other end. The tank being closed, by supplying air pressure on'the surface of the liquor therein, the drip liquor can be forced back into the -preheater through pipe 20.

At 21 is shown an acid gas supply pipe,-

designed' to conduct the acid gases resulting from the roasting of 'pyritic ores, these gases containing principally sulfur dioxid, S0 and carbon dioxid, CO and sometimes some aquc ous vapor. The said pipe 21 enters into the first combining chamber 15, which consists of an outer casing 22 of wood or other suitable material, having a conical bottom provided with a draw-valve '24, by which the contents may be discharged into barrels or bags. Within this chamber is a silk, muslin, or burlap wall 25, and between said well and'the 1,0 grade (said pie-heater being of the type de- 1 side walls of the outer casing 22 is an annular consists of an outer casing 30 and an inner casing 31 of burlap, muslin, or the like, having a solid top 32 from which is hung a number of ropes 33. The uncombined gases passing through the walls 31 and up between the annular space between 30 and 31 flow through pipe 34 into chamber 17 where a fresh supply of ammonia is delivered through the end of pipe 14. This chamber is of substantially the same construction as chamber 15, the uncombined gases passing out through pipe 35 into chamber 18, which is identical in structure with chamber 16, and finally through pipe 36 to the washer 37 designed to collect any uncombined ammonia. The ammonia liquor from the washer 37 is collected in tank 38 and forced by air pressure, or in any other suitable manner, either to the pre-heater 5 or to the still 6, as may be desired. The am-.

Inonia gases containing some aqueous vapor delivered from pipe 14 and branch pipe 29 into the combining chamber 15 meet the ases containing S0 and CO as they issue l rom pipe 21, the volatile base, .ammoma, combining with the acid radical SO to form ammonium sulfite, as follows:

whichit-Ldepo'sit'ed in a fine powder, and may be subsequently converted into ammonium carbonate by treatment with superheated steam, or may be heated in retorts to decompose it into ammonium carbonate and.

urea by the following:

2NH .OO .NH (N H,),(] 0 CON 1d,.

The ammonia in the combining chamber 17 combines with the carbon dioxid for the reason that there is no sulfur dioxid, present, the

greater afiinity'of the latter for the former preventing the formation of carbamate in the first two chambers.

place of sulfurous acid gas, or the gas result ing from the roasting of pyritic ores, we may 'use hydrochloric acid gas to'produce chlorids. We may use volatilizable metals, such as lead and zinc, and thereby produce either chlorids or sulfates, depending upon the acid radical introduced and intended, to be ,combined.

Having thus described our invention, what we claim as new and desire to secure by Letters Patent is:

1. The method of producing salts, which comprises conducting sulfur dioxid and a suitable base in a gaseous state into a closed chamber in the presence of aqueous vapor in amount only sufiicient to effect their union as a powdered salt.

2. The method of producing salts, which comprises conducting anacid gas and a base in a gaseous state into a closed chamber in the presence of aqueous vapor, said base and acid gas being capable of combining to form a plurality of salts, and depositing one of said salts in said chamber and depositing another of said salts in another chamber.

3. The method of producing salts, which comprises conducting an acid gas and a volatilized base into a closed chamber in the presence of aqueous vapor in amount only sufiicient to cause the de osition of but one salt as a powder, and con noting the residual gases from said chamber for further treatment.

4. The method of producing salts, which comprises conducting an acid gas-and a base in a gaseous state into a closed chamber in the presence of aqueous vapor suflicient to deposit a salt as a powder, and conducting the residual gases into another closed chamher and reacting upon them with the same base to deposit another and different salt as a powder.

5. The method of producing salts, which comprises reacting in a closed chamber upon gases resulting from the roasting of pyrjtic ores, with ammonia gas, in the presence of aqueous vapor in amount only suflicient to cause the deposition of ammonium sulfite as a powder 6. The methcdpf producing salts, which comprises reacting in a closed chamber upon gases resulting from the roasting of pyritic ores, with ammonia, inithe presence of an aqueous vapor,- to form ammonium sulfite,

and reacting upon the residual gases containing carbon dioxid with ammonia to form set our hands in the presence of two subscribing witnesses.

TALMADGE 'BLAss; JACOB LUTHER HAEHNLEN. WALTER WETHERILL 00 Witnesses for Talmadge Blass: R. S. BRENNESHOLTZ,

F. H. BURNETT. Witnesses for Jacob Luther Walter Wetherill Cox:

EUGENE HoosTER, J. HENRY MILLER.

Haehnlen and 

